• Title/Summary/Keyword: pH standard solution

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Study on the Solid Phase Extraction of Hg(II)-SBDTR Chelate with C18 Disks and Its Application to the Determination of Mercury in Tobacco and Tobacco Additive

  • Yang, Guan-Gyu;Xia, Zhen-Yuang;Wu, Yu-Ping;Sun, Han-Dong;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.549-552
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    • 2004
  • A sensitive, selective and rapid method has been developed for the determination of mercury based on the rapid reaction of mercury(II) with p-sulfobenzylidenethiorhodanine (SBDTR) and the solid phase extraction of the colored chelate with $C_{18}$ disks. In the presence of pH 3.5 sodium acetate-acetic acid buffer solution and Emulsifier-OP medium, SBDTR reacts with mercury(II) to form a red chelate of a molar ratio 1 : 2 (mercury to SBDTR). This chelate was prconcentrated by solid phase extraction with $C_{18}$ disks. An enrichment factor of 50 was achieved. The molar absorptivity of the chelate is $1.28{\times}10^5 L{\cdot}mol^{-1}{\cdot}cm^{-1}$ at 545 nm in measured solution. Beer's law is obeyed in the range of 0.01-3 ${\mu}$g/mL. The relative standard deviation for eleven replicates sample of 0.01 ${\mu}$g/mL is 1.65%. This method was applied to the determination of mercury in tobacco and tobacco additive with good results.

Method for Rapid Determination and Removal of Nitrogen Oxides in Flue Gases (Ⅰ). Rapid Determination on Nitrogen Oxides (배기가스중 질소산화물의 신속측정법과 그 제거에 관한 연구 (제1보). NO$_x$의 신속 정량법)

  • Yong Keun Lee;Tong Oh Seo;Kee Jung Paeng;Man Koo Kim;Kyu Ja Whang
    • Journal of the Korean Chemical Society
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    • v.29 no.1
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    • pp.52-60
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    • 1985
  • Oxides of nitrogen (NO$_x$) in exhaust gases was determined by absorbing the gas in alkaline peroxide solution containing 0.03${\%}$ H2O2 and 0.1N NaOH. About 100 ppm of NO$_x$ was rapidly oxidized to NO$_2$ or N$_2$O$_5$ by H$_2$O$_2$ and required a contact time of 2 minutes with the absorbing solution for complete absorption. With vigorous shaking including air or oxygen gas, high concentration of NO$_x$ (>200 ppm) can be absorbed within 30 minutes. The remaining H$_2$O$_2$ affect the absorbance of color solution strongly. However, the excess H$_2$O$_2$ was completely decomposed by zinc powder 0.5g and the sample solution should be adjusted to the pH range 6.1∼6.6 before the reduction so that conversion of nitrate to nitrite ion is possible. The absorbed NO$_x$ is determined colorimetrically by the diazotization-coupling method with sulfonilamide and NEDA as the coupling agent. The sensitivity of the new method was 4.48 ${\times}$ 10$^4$ as molar absorptivity which was high sensitive compared with that obtained for the usual zinc reduction NEDA method with O$_3$. This method was far more rapid, brief and accurate than previously published O$_3$-NEDA method in Korean industrial standard.

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Study on Solvent Extraction Using Salen(NEt2)2 as a Chelating Agent for Determination of Trace Cu(II), Mn(II), and Zn(II) in Water Samples

  • In, Gyo;Kim, Young-Sang;Choi, Jong-Moon
    • Bulletin of the Korean Chemical Society
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    • v.29 no.5
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    • pp.969-973
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    • 2008
  • Solvent extraction using a Schiff-base, salen$(NEt_2)_2$, as a chelating agent has been conducted on several water samples to study the determination of trace Cu(II), Mn(II) and Zn(II). Experimental conditions for the formation and extraction of metal complexes were optimized with an aqueous solution similar in composition to the samples. The matrix difference between the sample and standard solutions was approximately matched, and the pH of each sample solution was adjusted to 9.5 with $NaHCO_3/NaOH$ buffer. The concentration of salen$(NEt_2)_2$ was $7.3\;{\times}\;10^{-3}$ mol/L, and the complexes were extracted into MIBK solvent followed by the measurement of AAS absorbance. The potential interference of concomitant ions was investigated, but no interference from alkaline and alkali earth ions was shown in this procedure. The given procedure is precise, as judged from the relative standard deviation of less than 5% for five measured data. The recovery of 93-103% shows that this method is quantitative for such trace metal analysis.

Studies of Magnesium-Eriochrome Black T Complex in Acetonitrile (Acetonitrile에서의 Mg-EBT$^-$ 착물에 관한 연구)

  • Doo Won Park;Won Hyung Choi;Heung Lark Lee
    • Journal of the Korean Chemical Society
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    • v.17 no.4
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    • pp.256-261
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    • 1973
  • Complex formation of magnesium-Eriochrome Black T at constant ionic strength and hydrogen ion concentration have been studied spectrophotometrically in acetonitrile solution. The measured pH values were calibrated with standard buffer solutions by using a glass electrode Ag/0.1M $AgNO_3$ reference electrode couple. The results are as follows;$E_{glass}=716+59.1\;logA_{H+}[mv]$+(in mv. vs. Ag reference electrode for picric acid $-10^{-3}M$ tetramethylammonium picrate buffer), and $E_{glass}=1,193+59.1\;logA_{H+}[mv]$(in mv. vs. Ag reference electrode for 1,3-diphenylguanidine $-3{\times}10^{-3}M $ 1,3-diphenylguanidine perchlorate buffer). The acid dissociation exponent of ligand, $ pK_{H,EBT-}$was found to be 9.1. The conditional formation constants of $MgEBT^{-}$complex by log-ratio method were 3.97 (when m = 2) and 5.02 (when m = 1) as $log K_n$, respectively, for the reaction of $H_mEBT^{(3-m)-} + Mg^{2+} {\leftrightarrow}MgEBT^{-} + mH^{+}$. The present study showed that$MgEBT^{-}$ has the composition of 1:1 which agrees with the result of Schwarzenbach et al. in aqueous solution.

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Study on the Re-corrosion Characteristics of Corrosion Products by Weeping of Iron Artifacts (철제유물 Weeping에 따른 부식화합물의 재부식 특성 연구)

  • Park, Hyung-Ho;Lee, Hye-Youn;Lee, Jae-Sung;Yu, Jae-Eun
    • Journal of Conservation Science
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    • v.29 no.3
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    • pp.287-296
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    • 2013
  • Excavated iron objects are preserved in stable condition through processes of conservation treatment because they are found in the form of various corrosion products. However, the conservation treatment leads to re-corrosion over time and accordingly, iron objects can be severely damaged, and therefore fundamental measures need to be prepared to control it. In this study, the types and characteristics of corrosion products were scientifically analyzed according to the re-corrosion of iron artifacts. In addition, the stability of the corrosion products was evaluated by exposing the standard samples under the re-corrosion environment. Re-corrosion proceeded with weeping in reddish brown on the cracks of iron artifacts. Weeping was detected akagan$\acute{e}$ite had a low hydrogen ion concentration and high chloride ion. The selection of standard sample goethite, lepidocrocite, hematite, and magnetite, were evaluated corrosive by weeping. After the samples were immersed in HCl(pH 1), $H_2SO_4$(pH 1), $H_2O$(pH 6) solution, they had been maintained for 180 days in relative humidity of 20%, 50%, 80% to investiage the changes of chemical components. As a result of analysis, the changes of chemical components were not showed in goethite, lepidocrocite, and hematite. But magnetite was changed to lepidocrocite in solution including chloride ion($Cl^-$) and to goethite and lepidocrocite solution including sulfuric acid($SO{_4}^{2-}$). Results of the study, in the case of magnetite known as s stable corrosion compound, it was identified the corrosion of magnetite occurs by corrosive ions, which means weeping generated in the iron artifacts can corrode magnetite as well as base metal.

The Study on the Separation of the Subsidiary Elements in Iron and Steel by Using Ion Exchangers (II). The Separation of Anions (이온 교환수지에 의한 철 및 강의 분석에 관한 연구 (제2보). 음이온 성분의 분리)

  • Byoung-Cho Lee;Myon-Yong Park;Kee-Chae Park
    • Journal of the Korean Chemical Society
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    • v.17 no.6
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    • pp.428-433
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    • 1973
  • The quantitative separations of a mixture containing equal amount of each anion such as Si(IV), As(V), P(V), S(VI), W(VI) and Cr(VI) are carried out by the elution through 20${\times}3.14cm^2$ column of anion exchange resin, Dowex 1${\times}$8. The eluents are a mixture of 0.07 M hydrochloric acid and 0.03 M sodium chloride (pH = 1.30) for Si(IV), As(V) and P(V) species, a mixture of 0.6 M sodium chloride and 0.3 M sodium hydroxide for S(VI), W(VI) and Cr(VI) species, and 0.1 N sodium sulfite (pH = 3.48) for P(V) and As(V) species. The subsidiary anions in a standard mixture such as Si(IV), As(V), S(VI), P(V) and W(VI) are separated together from large amount of Fe(III) by the elution through 30cm${\times}3.14cm^2$ column of the resin, Dowex${\times}$50w${\times}$12, using a mixture of 0.1 M sodium nitrate and 2 percent dimethylsulfoxide aqueous solution as an eluent. Si(IV), As(V), S(VI), P(V) and W(VI) eluted together are separated quantitatively under the same conditions as in the separations of the anion mixture. By the conditions obtained in the separations of the standard mixture, Fe(III) and all of the subsidiary anions in steel are quantitatively separated.

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Determination of Boron Steel by Isotope-Dilution Inductively Coupled Plasma Mass Spectrometry after Matrix Separation

  • Park, Chang-J.
    • Bulletin of the Korean Chemical Society
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    • v.23 no.11
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    • pp.1541-1544
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    • 2002
  • The concentration of B in steels is important due to its influence on mechanical properties of steel such as hardenability, hot workability, and creep resistance. An analytical method has been developed to determine B in steel samples by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). National Institute of Standard and Technology Standard Reference Material (NIST SRM) 348a was analyzed to validate the analytical method. The steel sample was digested in a centrifuge bottle with addition of aqua regia and $^{10}B$ spike isotope. Sample pH was then adjusted to higher than 10 to precipitate most matrix elements such as Fe, Cr, and Ni. After centrifugation, the supernatant solution was passed through a cation exchange column to enhance the matrix separation efficiency. B recovery efficiency was about 37%, while matrix removal efficiency was higher than 99.9% for major matrix elements. The isotope dilution method was used for quantification and the determined B concentration was in good agreement with the certified value.

Quantitation and Validation of Atorvastatin using HPLC-UV

  • Heine, Daniel;Yong, Chul-Soon;Kim, Jung-Sun
    • Journal of Pharmaceutical Investigation
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    • v.37 no.3
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    • pp.187-192
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    • 2007
  • A reversed phase HPLC analysis of atorvastatin (AS) standard solution was performed using diclofenac (DF) as internal standard. Column oven temperature, flow rate and the composition of the mobile phase were varied in order to determine a practical system setup using a C18 column and UV detector. Two C18 columns of different length were compared regarding their influence on the AS peak shape. Based on these preliminary experiments a validation study was performed utilizing a C18 column at $62^{\circ}C$ with a mobile phase consisting of sodium phosphate buffer (0.05 M, pH 4.0), methanol and acetonitrile (40:50:10, v/v/v). The detection limit for AS was $0.1{\mu}g/ml$ and inter- and intra-day calibration curves were linear over a concentration range of $0.2-50{\mu}g/ml$. Accuracy and precision were satisfactory in the AS concentration range of $0.5-50{\mu}g/ml$.

Handling a Multi-Tasking Environment via the Dynamic Search Genetic Algorithm

  • Koh, S.P.;Aris, I.B.;Bashi, S.M.;Chong, K.H.
    • Journal of Electrical Engineering and Technology
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    • v.3 no.1
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    • pp.125-129
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    • 2008
  • A new genetic algorithm for the solution of a multi-tasking problem is presented in this paper. The approach introduces innovative genetic operation that guides the genetic algorithm more directly towards better quality of the population. A wide variety of standard genetic parameters are explored, and results allow the comparison of performance for cases both with and without the new operator. The proposed algorithm improves the convergence speed by reducing the number of generations required to identify a near-optimal solution, significantly reducing the convergence time in each instance.

The Microstructure and Magnetic Properties of YIG Powders Synthesized by a Coprecipitaion and a Sonochemical Process

  • Hong, Seong-Min;Kim, Yong-Il;Kim, Cheol-Gi
    • Journal of Magnetics
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    • v.14 no.4
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    • pp.165-167
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    • 2009
  • Nano-sized Yttrium iron garnet (YIG;$Y_3Fe_5O_{12}$) particles have been synthesized by using coprecipitation and a heat treatment process. The YIG particles were made using a nitrate or a chloride salt solution. The pH concentration of the solution was fixed at 12. Spherical shaped YIG particles were made with a size of about 20 nm. The magnetization value of the particles was smaller than the bulk value but their coercive field showed a high value.